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Method for separating and analyzing avenanthramide D and dihydroavenanthramide D

A technology for separation and analysis of avenanthramide, which is applied in the field of chemical substance analysis and separation, can solve problems such as small difference and achieve the effect of a reliable method

Active Publication Date: 2018-04-20
福州美乐莲生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, although the molecular weights of avenal alkaloid D and its selective hydrogenation product dihydroavenine D are large, the difference is very small, and the structure is basically the same, so there is a small difference in polarity

Method used

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  • Method for separating and analyzing avenanthramide D and dihydroavenanthramide D
  • Method for separating and analyzing avenanthramide D and dihydroavenanthramide D
  • Method for separating and analyzing avenanthramide D and dihydroavenanthramide D

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Instrument: ULtimate 3000 high performance liquid chromatography; UV detector

[0025] Chromatographic column: chiral HDL column (β-cyclodextrin as stationary phase)

[0026] Mobile phase: main mobile phase: 30% acetonitrile, 70% water (0.3% triethylamine, 0.3% glacial acetic acid), the water of 560mL, the acetonitrile of 240mL, the triethylamine of 1.7mL, the glacial acetic acid of 1.7mL are mixed, Ultrasonic degassing for 30min. Placed in the chromatographic inlet;

[0027] Mobile phase flow rate: 0.8mL / min

[0028] Detection wavelength: 254nm

[0029] Column temperature: 30°C

[0030] Injection volume: 0.8uL

[0031] Test procedure: Weigh 10mg of oat alkaloid raw material powder, put it in a 50mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, take 20mL precisely, put it in a 25mL sample bottle, shake well, as the raw material sample solution, place in the autosampler tray.

[0032] Set the detection method and sequence: the autom...

Embodiment 2

[0034] Instrument: ULtimate 3000 high performance liquid chromatography; UV detector

[0035] Chromatographic column: chiral HDL column (β-cyclodextrin as stationary phase)

[0036] Mobile phase: main mobile phase: 30% acetonitrile, 70% water (0.3% triethylamine, 0.3% glacial acetic acid), the water of 560mL, the acetonitrile of 240mL, the triethylamine of 1.7mL, the glacial acetic acid of 1.7mL are mixed, Ultrasonic degassing for 30min. Placed in the chromatographic inlet.

[0037] Flow rate: 0.8mL / min

[0038] Detection wavelength: 254nm

[0039] Column temperature: 30°C

[0040] Injection volume: 0.8uL

[0041] Test procedure: Weigh 10 mg of standard dihydrooat alkaloid raw material powder, put it in a 50 mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, accurately measure 20 mL, place it in a 25 mL sample bottle, shake well, and use it as a raw material Sample solution, placed in the autosampler tray.

[0042] Set the detection method ...

Embodiment 3

[0044] Instrument: ULtimate 3000 high performance liquid chromatography; UV detector

[0045] Chromatographic column: chiral HDL column (β-cyclodextrin as stationary phase)

[0046] Mobile phase: main mobile phase: 30% acetonitrile, 70% water (0.3% triethylamine, 0.3% glacial acetic acid), the water of 560mL, the acetonitrile of 240mL, the triethylamine of 1.7mL, the glacial acetic acid of 1.7mL are mixed, Ultrasonic degassing for 30min. Placed in the chromatographic inlet.

[0047] Flow rate: 0.8mL / min

[0048] Detection wavelength: 254nm

[0049] Column temperature: 30°C

[0050] Injection volume: 0.8uL

[0051] Test procedure: Weigh 10 mg of the mixed sample of avena alkaloid D and standard dihydroavenine D, put them together in a 50mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, accurately measure 20mL and put it in a 25mL sample bottle, Shake well, and place it in the autosampler tray as the raw sample solution.

[0052] Set the det...

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Abstract

The invention discloses a method for separating and analyzing avenanthramide D and dihydroavenanthramide D. High performance liquid chromatography is adopted, the chromatographic column is a chiral chromatographic column with cyclodextrin as a stationary phase, the mobile phase is composed of an organic phase and an aqueous phase according to a volume ratio of (25-30):(70-75), the organic phase ismethanol, ethanol, acetonitrile or tetrahydrofuran, the aqueous phase adopts water as a solvent and contains 0.1-1 V% of a buffer agent and 0.1-1 V% of a pH adjuster, the buffer agent is triethylamine phosphate, triethylamine acetate or triethylamine, and the pH adjuster is glacial acetic acid or phosphoric acid; and the automatic injection volume is 0.5 [mu]L, the flow rate of the mobile phase is 0.5-1.5 mL / min, the detection wavelength was 254 nm, and the column temperature is 30 DEG C. The invention provides the reliable method for accurately completing the analysis and separation of the avenanthramide D and its hydrogenation product dihydroavenanthramide D by selecting the appropriate stationary phase, the appropriate mobile phase and appropriate determination conditions.

Description

technical field [0001] The invention belongs to the technical field of analysis and separation of chemical substances, and in particular relates to a method for separation and analysis of avenal alkaloid D and dihydroavenic alkaloid D. Background technique [0002] Oat alkaloid D, as the only phenolic compound found in oats, has certain biological activities due to the functional amide bond contained in its structure: hypoglycemic, hypolipidemic, antioxidant, anti-inflammatory, vasodilation, Anti-proliferation and antipruritic etc. CN106511110A discloses that dihydroavenine D is a raw material for synthesizing dihydroavenine D salt compounds, and the dihydroavenine D salt compounds are active ingredients of cosmetics. The selective hydrogenation of C=C double bond of avenantine alkaloids to synthesize dihydroavenine D is an important synthetic process, in which the separation and analysis of raw materials and products are indispensable means. [0003] The structural formul...

Claims

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Application Information

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IPC IPC(8): G01N30/02B01D15/38B01D15/10
Inventor 陈秉辉张蕾郑进保胡涛张诺伟叶松寿谢建榕
Owner 福州美乐莲生物科技有限公司
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